CN110455445B - Flexible stress sensor and preparation method thereof - Google Patents
Flexible stress sensor and preparation method thereof Download PDFInfo
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- CN110455445B CN110455445B CN201910653791.0A CN201910653791A CN110455445B CN 110455445 B CN110455445 B CN 110455445B CN 201910653791 A CN201910653791 A CN 201910653791A CN 110455445 B CN110455445 B CN 110455445B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/02—Detecting, measuring or recording pulse, heart rate, blood pressure or blood flow; Combined pulse/heart-rate/blood pressure determination; Evaluating a cardiovascular condition not otherwise provided for, e.g. using combinations of techniques provided for in this group with electrocardiography or electroauscultation; Heart catheters for measuring blood pressure
- A61B5/024—Detecting, measuring or recording pulse rate or heart rate
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/02—Detecting, measuring or recording pulse, heart rate, blood pressure or blood flow; Combined pulse/heart-rate/blood pressure determination; Evaluating a cardiovascular condition not otherwise provided for, e.g. using combinations of techniques provided for in this group with electrocardiography or electroauscultation; Heart catheters for measuring blood pressure
- A61B5/024—Detecting, measuring or recording pulse rate or heart rate
- A61B5/02444—Details of sensor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01H—MEASUREMENT OF MECHANICAL VIBRATIONS OR ULTRASONIC, SONIC OR INFRASONIC WAVES
- G01H11/00—Measuring mechanical vibrations or ultrasonic, sonic or infrasonic waves by detecting changes in electric or magnetic properties
- G01H11/06—Measuring mechanical vibrations or ultrasonic, sonic or infrasonic waves by detecting changes in electric or magnetic properties by electric means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/02—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
- G01L9/04—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning of resistance-strain gauges
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Abstract
The invention provides a flexible stress sensor and a preparation method thereof, wherein the flexible stress sensor comprises a strain sensing layer, an electrode and a flexible packaging layer, the strain sensing layer is electrically connected with the electrode, the flexible packaging layer comprises an upper PDMS substrate and a lower PDMS substrate and covers the strain sensing layer and the electrode, the electrode comprises silver paste and a lead, one end of the lead is bonded on the strain sensing layer through the silver paste, the other end of the lead is led to the outside of the flexible packaging layer, and the strain sensing layer is redox graphene with a prismatic net structure after laser reduction. Compared with the prior art, the invention has the advantages of good durability, large strain range during stretching, high sensitivity and linear and stable change.
Description
Technical Field
The invention relates to a flexible stress sensor and a preparation method thereof, belonging to the field of sensors.
Background
With the technical development of stress sensors, people have increasingly growing technical demands on real-time medical monitoring, bio-integrated therapy, wearable displays and lightweight mobile electronic devices. Compared with rigid carriers such as glass or silicon wafers, flexible electronic devices are electronic devices constructed on flexible polymers (e.g., polyethylene terephthalate (PET), polyethylene imine (PEI), or Polydimethylsiloxane (PDMS)), and since such flexible polymers exhibit elasticity, electronic elements on flexible polymer substrates can be bent and uniformly stretched, thereby being widely applied to various aspects such as deformable touch screens, biological recognition devices, wearable supercapacitors, or solar cells.
At present, the graphene oxide (RGO) is reduced by a chemical method and is used as a strain sensing material to prepare a flexible stress sensor, the linearity of the flexible stress sensor is poor, and the graphene oxide reduced by laser is used as the flexible stress sensor of the sensing material, no matter an etched film or a strip is easy to break under strain, so the strain range is small and the stability is poor.
In view of the above, it is necessary to provide a flexible stress sensor and a method for manufacturing the same to solve the above problems.
Disclosure of Invention
The invention aims to provide a flexible stress sensor and a preparation method thereof, which can realize linear change with large strain range, high sensitivity and stability.
In order to achieve the above object, the present invention provides a flexible stress sensor, which includes a strain sensing layer, an electrode and a flexible packaging layer, and is characterized in that: the strain induction layer is electrically connected with the electrode, the flexible packaging layer comprises an upper PDMS substrate and a lower PDMS substrate and covers the strain induction layer and the electrode, the electrode comprises silver paste and a lead, one end of the lead is bonded on the strain induction layer through the silver paste, the other end of the lead is led to the outside of the flexible packaging layer, and the strain induction layer is redox graphene with a prismatic net structure after laser reduction.
Optionally, the length of the strain sensing layer is 4mm-60mm, the width is 2mm-15mm, and the thickness is 0.2mm-2 mm.
Optionally, the acute angle of the prismatic net structure is 45-60 degrees, and the edge length is 100-700 μm.
Optionally, the redox graphene is a material obtained after two times of laser reduction.
Optionally, the sensitivity coefficient of the redox graphene is 35, and the strain range in stretching is at most 24%.
Optionally, the flexible encapsulation layer is made of a thermoplastic high molecular polymer.
Optionally, the thermoplastic high molecular polymer includes polyethylene terephthalate, polyethyleneimine, polydimethylsiloxane, polyurethane, polypropylene, or polytetrafluoroethylene.
In order to achieve the above object, the present invention further provides a method for manufacturing a flexible stress sensor, which is characterized by mainly comprising the following steps:
step S1, preparing GO aqueous solution as an initial raw material by adopting a Hummers method;
step S2, coating the GO aqueous solution on a lower-layer PDMS substrate, and naturally drying the GO aqueous solution to form a film;
step S3, placing the lower PDMS substrate coated with the GO film under a laser to obtain the redox graphene in a specified shape;
and S4, arranging electrodes on the redox graphene, and insulating and packaging the redox graphene and the electrodes by adopting an upper PDMS substrate.
Optionally, step S3 specifically includes:
s31, placing the lower PDMS substrate coated with the GO film under a laser, and printing for 5 minutes according to a laser printing pattern;
and S32, changing the laser scanning direction, carrying out laser second reduction again, and obtaining reduced redox graphene with a prismatic net structure after 5 minutes of laser printing.
Optionally, the packaging process in step S4 includes the following steps:
coating silver paste on the edges of two ends of the redox graphene, leading out a lead, drying for 5-10 min, and placing in a round vessel;
respectively measuring polydimethylsiloxane PDMS and a curing agent for mixing, wherein the volume ratio of the polydimethylsiloxane PDMS to the curing agent is 10: 1;
step (c), placing the polydimethylsiloxane PDMS solution prepared in the step (b) on a whirl coating table, and rotating at a high speed for 5 minutes to obtain a bubble-free solution of the polydimethylsiloxane PDMS;
and (d) pouring the bubble-free solution of the polydimethylsiloxane PDMS in the step (c) into a round vessel, putting the round vessel into an oven, curing the round vessel for 24 hours at the temperature of 60 ℃, meanwhile, packaging the redox graphene, the silver paste and the lead, and demolding after curing to obtain the flexible stress sensor.
The invention has the following beneficial effects: according to the method, graphene oxide with low cost is reduced by a physical laser method, so that the reduced graphene oxide with a prismatic net structure after laser reduction twice is obtained; meanwhile, the prismatic net-shaped redox graphene is packaged by the flexible packaging layer, so that the packaging structure is good in durability, large in strain range during stretching, high in sensitivity, linearly and stably changed, light in weight and strong in environmental adaptability, and can be flexibly and conveniently attached to the surfaces of various shapes.
Drawings
Fig. 1 is a schematic structural view of a flexible stress sensor of the present invention.
Fig. 2 is a schematic plan view of the PDMS substrate of fig. 1 with the upper layer removed.
Fig. 3 is a graph showing the relative resistance change of the redox graphene having a prismatic network structure under different stresses according to the present invention.
Fig. 4 is a test circuit diagram of the flexible stress sensor of the present invention for detecting signals.
FIG. 5 is a graph of the pulse beat signal measured by the test circuit of FIG. 4.
Fig. 6 is a graph of the throat vocalization signal measured by the test circuit of fig. 4.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
As shown in fig. 1 and 2, the present invention provides a flexible stress sensor, which includes a strain sensing layer, an electrode, and a flexible encapsulation layer, wherein the strain sensing layer is electrically connected to the electrode, and the flexible encapsulation layer includes an upper PDMS substrate and a lower PDMS substrate, and covers the strain sensing layer and the electrode.
The strain induction layer is redox graphene with a prismatic net structure after laser reduction, and the redox graphene is a material after two times of laser reduction.
The electrode comprises silver paste and a lead, one end of the lead is bonded on the strain sensing layer through the silver paste, and the other end of the lead is led to the outside of the flexible packaging layer.
The length of the strain sensing layer is 4mm-60mm, the width is 2mm-15mm, and the thickness is 0.2mm-2 mm.
The acute angle of the prismatic net structure is 45-60 degrees, and the edge length is 100-700 μm.
The flexible packaging layer is made of thermoplastic high molecular polymer, and the thermoplastic high molecular polymer comprises polyethylene glycol terephthalate, polyethyleneimine, polydimethylsiloxane, polyurethane, polypropylene or polytetrafluoroethylene.
The invention also provides a preparation method of the flexible stress sensor, which mainly comprises the following steps:
step S1, preparing GO aqueous solution as an initial raw material by adopting a Hummers method;
step S2, coating the GO aqueous solution on a lower-layer PDMS substrate, and naturally drying the GO aqueous solution to form a film;
step S3, placing the lower PDMS substrate coated with the GO film under a laser to obtain the redox graphene in a specified shape;
and S4, arranging electrodes on the redox graphene, and insulating and packaging the redox graphene and the electrodes by adopting an upper PDMS substrate.
Steps S1-S4 are explained in detail below.
In step S1, the specific steps of preparing the GO aqueous solution include:
(1) 23ml of concentrated sulfuric acid is taken in a dry beaker, and 1g of graphite powder and 3g of KMNO are added4Controlling the temperature of the reaction liquid not to exceed 10 ℃ and stirring;
(2) placing the beaker in 35 deg.C constant temperature water solution, performing ultrasound, and adjusting ultrasound frequency (60kHZ, 70kHZ, 80kHZ) and ultrasound time (10min, 20min, 30 min);
(3) adding 7ml deionized water into the same frequency ultrasound, controlling the reaction temperature at 100 ℃, performing ultrasound for 15min, and finally dropwise adding 30% of H2O2Solution until the reaction solution turns brown or yellow;
(4) the solution was centrifuged and washed thoroughly with 5% HCl and deionized water until the solution was free of SO4 2-When present, the final GO aqueous solution with concentration of 2mg/ml is obtained.
Step S3 specifically includes:
step S31, placing the lower PDMS substrate coated with the GO film under a laser, controlling a laser printing pattern by matching with a pattern input software Nero Start Smart running on a computer, leading a rectangle of 30mm x 10mm into the software, controlling the power of the laser to be 20%, the scanning speed of the laser to be 500mm/min, the line spacing of the laser printing to be 80-600 μm, controlling the scanning direction of the laser, and printing for 5 minutes by using the laser;
and S32, changing the laser scanning direction, keeping other conditions unchanged, performing laser secondary reduction again, and obtaining reduced redox graphene with a prismatic net structure after laser printing for 5 minutes.
As shown in fig. 3, it was detected that, in the case of changing the laser scanning direction, the sensitivity coefficient of the redox graphene having a prismatic network structure obtained by two times of laser reduction was 35, and the strain range was 24% at maximum when it was stretched.
The rated power of the laser beam in step S3 is 4W.
The sensitivity coefficient can be calculated by the following method: packaging the redox graphene prepared in the step S3 into a film sample by using polydimethylsiloxane PDMS, clamping the film sample on two sides of an electric displacement table, reading the moving distance of the displacement table, measuring the real-time resistance of the film sample by using a digital source table, and then calculating according to the following formula to obtain the redox graphene:
wherein GF represents a sensitivity coefficient; r represents an initial resistance (Ω); Δ R represents a relative resistance change (Ω); l represents an initial length (m); Δ L represents a relative length change (m).
In step S4, taking polydimethylsiloxane PDMS as an example, the specific steps of the encapsulation process of the flexible encapsulation layer include:
coating silver paste on the edges of two ends of the redox graphene, leading out a lead, drying for 5-10 min, and placing in a round vessel;
respectively measuring polydimethylsiloxane PDMS and a curing agent for mixing, wherein the volume ratio of the polydimethylsiloxane PDMS to the curing agent is 10: 1;
step (c), placing the polydimethylsiloxane PDMS solution prepared in the step (b) on a whirl coating table, and rotating at a high speed for 5 minutes to obtain a bubble-free solution of the polydimethylsiloxane PDMS;
and (d) pouring the bubble-free solution of the polydimethylsiloxane PDMS in the step (c) into a round vessel, putting the round vessel into an oven, curing the round vessel for 24 hours at the temperature of 60 ℃, meanwhile, packaging the redox graphene, the silver paste and the lead, and demolding after curing to obtain the flexible stress sensor.
The flexible stress sensor can be widely applied to the fields of heartbeat monitoring, pulse wave detection or sound signal acquisition and identification and the like. The following will exemplify heartbeat monitoring and pulse wave detection.
As shown in FIG. 4, the test circuit is composed of a constant voltage source Vs(10V), protective resistor R (100k omega), stress sensor resistor RGStress sensor resistor R formed with oscilloscopeGVoltage V acrossGComprises the following steps:
the voltage VGThe heartbeat or pulse signal can be reflected.
The flexible stress sensor prepared by the preparation method is attached to the wrist and throat of a human body and is tested by using the test circuit shown in figure 4.
Fig. 5 shows a graph of the measured pulse vibration signals. As shown in fig. 6, a plot of the measured throat vocalization signal.
As can be seen from fig. 5 and 6: the flexible stress sensor of the invention has greatly improved performances in the aspects of sensitivity, detection range and the like.
In conclusion, the graphene oxide with low cost is reduced by a physical laser method to obtain the laser-reduced graphene oxide with a prismatic net structure; meanwhile, the prismatic net-shaped redox graphene is packaged by the flexible packaging layer, so that the packaging structure is good in durability, large in strain range during stretching, high in sensitivity, linearly and stably changed, capable of being flexibly and conveniently attached to the surfaces of various shapes, light in weight and high in environmental adaptability.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the present invention.
Claims (9)
1. A flexible stress sensor comprises a strain sensing layer, an electrode and a flexible packaging layer, and is characterized in that: the strain sensing layer is electrically connected with the electrode, the flexible packaging layer comprises an upper PDMS substrate and a lower PDMS substrate and covers the strain sensing layer and the electrode, the electrode comprises silver paste and a lead, one end of the lead is bonded on the strain sensing layer through the silver paste, the other end of the lead is led to the outside of the flexible packaging layer, the strain sensing layer is redox graphene which is subjected to laser reduction and has a prismatic net structure, the acute angle of the prismatic net structure is 45-60 degrees, the thickness of the strain sensing layer is 0.2-2 mm, and the redox graphene is a material which is subjected to laser reduction twice.
2. The flexible stress sensor of claim 1, wherein: the length of the strain sensing layer is 4mm-60mm, and the width of the strain sensing layer is 2mm-15 mm.
3. The flexible stress sensor of claim 1, wherein: the edge length of the prismatic net structure is 100-700 mu m.
4. The flexible stress sensor of claim 1, wherein: the sensitivity coefficient of the redox graphene is 35, and the maximum strain range in stretching is 24%.
5. The flexible stress sensor of claim 1, wherein: the flexible packaging layer is made of thermoplastic high-molecular polymer.
6. The flexible stress sensor of claim 5, wherein: the thermoplastic high molecular polymer comprises polyethylene glycol terephthalate, polyethyleneimine, polydimethylsiloxane, polyurethane, polypropylene or polytetrafluoroethylene.
7. A method for manufacturing a flexible stress sensor according to any one of claims 1 to 6, comprising essentially the steps of:
step S1, preparing GO aqueous solution as an initial raw material by adopting a Hummers method;
step S2, coating the GO aqueous solution on a lower-layer PDMS substrate, and naturally drying the GO aqueous solution to form a film;
step S3, placing the lower PDMS substrate coated with the GO film under a laser to obtain the redox graphene in a specified shape;
and S4, arranging electrodes on the redox graphene, and insulating and packaging the redox graphene and the electrodes by adopting an upper PDMS substrate.
8. The method for manufacturing a flexible stress sensor according to claim 7, wherein the step S3 is specifically:
s31, placing the lower PDMS substrate coated with the GO film under a laser, and printing for 5 minutes according to a laser printing pattern;
and S32, changing the laser scanning direction, carrying out laser second reduction again, and obtaining reduced redox graphene with a prismatic net structure after 5 minutes of laser printing.
9. The method for manufacturing a flexible stress sensor according to claim 7, wherein the packaging process in step S4 comprises the following steps:
coating silver paste on the edges of two ends of the redox graphene, leading out a lead, drying for 5-10 min, and placing in a round vessel;
respectively measuring polydimethylsiloxane PDMS and a curing agent for mixing, wherein the volume ratio of the polydimethylsiloxane PDMS to the curing agent is 10: 1;
step (c), placing the polydimethylsiloxane PDMS solution prepared in the step (b) on a whirl coating table, and rotating at a high speed for 5 minutes to obtain a bubble-free solution of the polydimethylsiloxane PDMS;
and (d) pouring the bubble-free solution of the polydimethylsiloxane PDMS in the step (c) into a round vessel, putting the round vessel into an oven, curing the round vessel for 24 hours at the temperature of 60 ℃, meanwhile, packaging the redox graphene, the silver paste and the lead, and demolding after curing to obtain the flexible stress sensor.
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| CN111307204A (en) * | 2019-11-28 | 2020-06-19 | 杭州电子科技大学 | Flexible multifunctional sensor |
| CN111017863B (en) * | 2019-12-11 | 2023-09-29 | 昆明理工大学 | Silicon-based reticular graphene MEMS sensor and preparation method thereof |
| CN111664974A (en) * | 2020-04-26 | 2020-09-15 | 太原理工大学 | Black phosphorus flexible stress sensor and preparation method thereof |
| CN111855036A (en) * | 2020-07-29 | 2020-10-30 | 观云(山东)智能科技有限公司 | Ultra-wide range flexible sensor, preparation method thereof and distributed pressure monitoring system |
| CN112146796A (en) * | 2020-09-17 | 2020-12-29 | 有研工程技术研究院有限公司 | Flexible stress sensor and preparation method thereof |
| CN112146797A (en) * | 2020-09-29 | 2020-12-29 | 有研工程技术研究院有限公司 | Mxene-based multifunctional flexible mechanical sensor and preparation method thereof |
| CN113865475A (en) * | 2021-09-23 | 2021-12-31 | 浙江大学 | Preparation method and application of bionic self-adaptive winding wearable sensor for monitoring diameter micro-change of plant stem |
| CN114608638A (en) * | 2022-03-10 | 2022-06-10 | 浙江理工大学 | Packaging method of flexible microelectronic sensor |
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